CN110405221A - A kind of method that DC arc plasma prepares refractory metal nano powder - Google Patents
A kind of method that DC arc plasma prepares refractory metal nano powder Download PDFInfo
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- CN110405221A CN110405221A CN201910763266.4A CN201910763266A CN110405221A CN 110405221 A CN110405221 A CN 110405221A CN 201910763266 A CN201910763266 A CN 201910763266A CN 110405221 A CN110405221 A CN 110405221A
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- metal nano
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- nano powder
- refractory metal
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- 239000003870 refractory metal Substances 0.000 title claims abstract description 30
- 239000011858 nanopowder Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000010891 electric arc Methods 0.000 claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 27
- 238000002161 passivation Methods 0.000 claims abstract description 23
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 17
- 239000010937 tungsten Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims description 16
- 239000008246 gaseous mixture Substances 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 abstract description 45
- 239000002245 particle Substances 0.000 abstract description 13
- 238000002360 preparation method Methods 0.000 abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 235000013339 cereals Nutrition 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of methods that DC arc plasma prepares refractory metal nano powder, belong to metal nano powder preparation technical field.For the present invention using pure tungsten stick as cathode, the metal bar of prefabricated metal nano powder is anode；Reaction chamber is vacuumized, plasma gas is then passed to, setting electric current and voltage carry out arc discharge, while controlling anode at the uniform velocity to rise and control electric arc spacing is 1 ~ 3 mm；Arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano powder of reaction chamber wall.Refractory metal nano powder of the present invention has relatively regular spherical structure, and partial size is small and even particle size distribution, dispersibility are preferable.The method of the present invention uses the mixed gas for being added to hydrogen as plasma gas, and arc zone temperature is high, and has the advantages such as arc stability is high, easy to operate, preparation cost is lower, product qualities are high, preparation process is environmentally friendly.
Description
Technical field
The present invention relates to a kind of methods that DC arc plasma prepares refractory metal nano powder, belong to metal nano powder
Preparation technical field.
Background technique
Refractory metal refers to that fusing point is higher than 1650 DEG C and has the metal of certain reserves, mainly there is tungsten, titanium, molybdenum etc..Due to its tool
There are high-melting-point and excellent electric conductivity, thermal conductivity and corrosion resistance.Not with the related applications such as thermal spraying, 3D printing field
Disconnected development, the requirement to refractory metal powder are also higher and higher.Nanoscale refractory metal powder particles diameter is smaller, and surface property is more excellent,
Sintering temperature can be effectively reduced, improve sintered body performance.Refractory metal nano powder is as a kind of nano material haveing excellent performance
And the extensive concern of researchers is received, but the preparation of high-quality refractory metal nano powder is still industrial problem.
Currently, the method for industrially preparing refractory metal nano powder mainly has high-energy ball milling method, evaporation and electronation
Method etc..But the refractory metal nano powder granularity that these methods are prepared is larger, purity is not high enough, and dispersibility is poor.
Summary of the invention
In view of the problems of the existing technology the present invention, provides a kind of DC arc plasma and prepares refractory metal nanometer
The method of powder, arc stability of the present invention is high, can prepare that purity is high, good dispersion, partial size be small and the difficulty of even particle size distribution
Molten metal nano powder, and can be by changing the experiment parameters such as plasma gas pressure, electric current, to refractory metal nano particle
Partial size and yield controlled.
A kind of method that DC arc plasma prepares refractory metal nano powder, the specific steps are as follows:
(1) using pure tungsten stick as cathode, metal bar of the fusing point higher than 1650 DEG C is anode；
(2) reaction chamber is vacuumized, then passes to plasma gas, setting electric current and voltage carry out arc discharge, same to time control
It is 1 ~ 3 mm that anode processed, which at the uniform velocity rises and controls electric arc spacing,；
(3) step (2) arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano of reaction chamber wall
Powder.
Further, step (1) anode is tungsten bar, molybdenum bar or stud.
The diameter of step (1) cathode is 10 ~ 20 mm, and 10 ~ 30 cm of length, the bottom end of cathode is cone structure.
Further, the diameter of step (1) anode is 10 ~ 20 mm, 10 ~ 30 cm of length.
Step (2) plasma gas is Ar/H2、N2/H2Or He/H2Gaseous mixture system, plasma gas stagnation pressure
Power is 60 ~ 80 kPa, H in plasma gas2Volume account for 1/3 ~ 1/2.
Further, step (2) electric current is 150-200 A, and voltage is 25-36 V, and the time of arc discharge is 5-
10 min。
Further, step (3) passivation gas is the air of 5 ~ 15 kPa, and passivation time is 8 ~ 10 h.
DC arc plasma principle: the arc discharge between electrode, which produces, reaches 104The high temperature of K makes to react
Gas transition in room is plasma state, and refractory metal anode is sublimed into rapidly gaseous atom；Then oversaturated infusibility gold
Belong to steam and flow to the lower position of temperature in reaction chamber, nucleating growth is at corresponding nano particle again.
The beneficial effects of the present invention are:
(1) the method for the present invention uses the mixed gas for being added to hydrogen as plasma gas, and arc zone temperature is high, and has
There are the advantages such as arc stability is high, easy to operate, preparation cost is lower, product qualities are high, preparation process is environmentally friendly；
(2) present invention control refractory metal anode at the uniform velocity rises, and keeps electrode spacing constant, is conducive to arc stability, so that difficult
Molten metal nano powder has relatively regular spherical structure, and partial size is small and even particle size distribution, dispersibility are preferable；
(3) present invention change electric current and plasma gas pressure can the partial size to product controlled with yield, can be with
Various sizes of product is prepared according to different demands；
(4) Passivation Treatment of the present invention can effectively reduce the activity of refractory metal nano powder, improve security performance.
Detailed description of the invention
Fig. 1 is the transmission electron microscope figure of nano-tungsten powder in embodiment 1；
Fig. 2 is the particle size distribution figure of nano-tungsten powder in embodiment 1；
Fig. 3 is the transmission electron microscope figure of nano Mo powder in embodiment 2；
Fig. 4 is the particle size distribution figure of nano Mo powder in embodiment 2.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
A kind of embodiment 1: method that DC arc plasma prepares refractory metal nano powder, the specific steps are as follows:
(1) using pure tungsten stick as cathode, the metal bar (tungsten bar) that 3410 DEG C of fusing point is anode, and metal bar (tungsten bar) anode is fixed on
In the hole slot of water jacketed copper crucible；Wherein the diameter of cathode is 10mm, and 10 cm of length, the bottom end of cathode is cone structure；Anode
Diameter is 10 mm, 10 cm of length；
(2) reaction chamber is vacuumized, then passes to plasma gas, setting electric current and voltage carry out arc discharge, same to time control
It is 1 ~ 3 mm that anode processed, which at the uniform velocity rises and controls electric arc spacing,；Wherein plasma gas is Ar/H2Gaseous mixture system, plasma
Body total gas pressure is 60 kPa, H in plasma gas2Volume account for 1/2；Electric current is 200 A, and voltage is 36 V, electric arc
The time of electric discharge is 5min；
(3) step (2) arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano of reaction chamber wall
Powder (nano-tungsten powder)；Wherein passivation gas is the air of 15 kPa, and passivation time is 10 h；
The transmission electron microscope figure of the present embodiment nano-tungsten powder is as shown in Figure 1, from fig. 1, it can be seen that nano-tungsten powder is with relatively regular
Spherical structure, even particle size distribution, dispersibility preferably；Fig. 2 is the particle size distribution figure of nano-tungsten powder, can be seen that and receives by 2 figures
For the partial size of rice tungsten powder between 10-40 nm, average grain diameter is 23.7 nm.
A kind of embodiment 2: method that DC arc plasma prepares refractory metal nano powder, the specific steps are as follows:
(1) using pure tungsten stick as cathode, the metal bar (molybdenum bar) that 2620 DEG C of fusing point is anode, and metal bar (molybdenum bar) anode is fixed on
In the hole slot of water jacketed copper crucible；Wherein the diameter of cathode is 10mm, and 20 cm of length, the bottom end of cathode is cone structure；Anode
Diameter is 10 mm, 20 cm of length；
(2) reaction chamber is vacuumized, then passes to plasma gas, setting electric current and voltage carry out arc discharge, same to time control
It is 1 ~ 3 mm that anode processed, which at the uniform velocity rises and controls electric arc spacing,；Wherein plasma gas is Ar/H2Gaseous mixture system, plasma
Body total gas pressure is 70 kPa, H in plasma gas2Volume account for 1/2；Electric current is 175A, voltage 30V, and electric arc is put
The time of electricity is 8min；
(3) step (2) arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano of reaction chamber wall
Powder (nano Mo powder)；Wherein passivation gas is the air of 10 kPa, and passivation time is 9 h；
The transmission electron microscope figure of the present embodiment nano Mo powder is as shown in figure 3, as can be seen from Figure 3, nano Mo powder has relatively regular
Spherical structure, even particle size distribution, dispersibility preferably；Fig. 4 is the particle size distribution figure of nano Mo powder, can be seen that and receives by 4 figures
For the partial size of rice molybdenum powder between 10-60 nm, average grain diameter is 27 nm.
A kind of embodiment 3: method that DC arc plasma prepares refractory metal nano powder, the specific steps are as follows:
(1) using pure tungsten stick as cathode, the metal bar (stud) that 1668 DEG C of fusing point is anode, and metal bar (stud) anode is fixed on
In the hole slot of water jacketed copper crucible；Wherein the diameter of cathode is 10mm, and 30 cm of length, the bottom end of cathode is cone structure；Anode
Diameter is 10 mm, 30 cm of length；
(2) reaction chamber is vacuumized, then passes to plasma gas, setting electric current and voltage carry out arc discharge, same to time control
It is 1 ~ 3 mm that anode processed, which at the uniform velocity rises and controls electric arc spacing,；Wherein plasma gas is Ar/H2Gaseous mixture system, plasma
Body total gas pressure is 80 kPa, H in plasma gas2Volume account for 1/3；Electric current is 150 A, and voltage is 25 V, electric arc
The time of electric discharge is 10min；
(3) step (2) arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano of reaction chamber wall
Powder (nano titanium powder)；Wherein passivation gas is the air of 5 kPa, and passivation time is 8 h；
The present embodiment nano titanium powder has relatively regular spherical structure, and even particle size distribution, dispersibility is preferably；The grain of nano titanium powder
For diameter between 15-60 nm, average grain diameter is 35 nm.
A kind of embodiment 4: method that DC arc plasma prepares refractory metal nano powder, the specific steps are as follows:
(1) using pure tungsten stick as cathode, the metal bar (tungsten bar) that 3410 DEG C of fusing point is anode, and metal bar (tungsten bar) anode is fixed on
In the hole slot of water jacketed copper crucible；Wherein the diameter of cathode is 20mm, and 20 cm of length, the bottom end of cathode is cone structure；Anode
Diameter is 20mm, 20 cm of length；
(2) reaction chamber is vacuumized, then passes to plasma gas, setting electric current and voltage carry out arc discharge, same to time control
It is 1 ~ 3 mm that anode processed, which at the uniform velocity rises and controls electric arc spacing,；Wherein plasma gas is N2/H2Gaseous mixture system, plasma
Body total gas pressure is 60 kPa, H in plasma gas2Volume account for 1/2；Electric current is 200 A, voltage 25V, and electric arc puts
The time of electricity is 6min；
(3) step (2) arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano of reaction chamber wall
Powder (nano-tungsten powder)；Wherein passivation gas is the air of 15 kPa, and passivation time is 10 h；
The present embodiment nano-tungsten powder has relatively regular spherical structure, and even particle size distribution, dispersibility is preferably；The grain of nano-tungsten powder
For diameter between 15-45 nm, average grain diameter is 29 nm.
A kind of embodiment 5: method that DC arc plasma prepares refractory metal nano powder, the specific steps are as follows:
(1) using pure tungsten stick as cathode, the metal bar (tungsten bar) that 3410 DEG C of fusing point is anode, and metal bar (tungsten bar) anode is fixed on
In the hole slot of water jacketed copper crucible；Wherein the diameter of cathode is 15mm, and 20 cm of length, the bottom end of cathode is cone structure；Anode
Diameter is 15mm, 20 cm of length；
(2) reaction chamber is vacuumized, then passes to plasma gas, setting electric current and voltage carry out arc discharge, same to time control
It is 1 ~ 3 mm that anode processed, which at the uniform velocity rises and controls electric arc spacing,；Wherein plasma gas is He/H2Gaseous mixture system, plasma
Body total gas pressure is 70kPa, H in plasma gas2Volume account for 1/2；Electric current is 175A, voltage 30V, arc discharge
Time be 8min；
(3) step (2) arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano of reaction chamber wall
Powder (nano-tungsten powder)；Wherein passivation gas is the air of 10 kPa, and passivation time is 9 h；
The present embodiment nano-tungsten powder has relatively regular spherical structure, and even particle size distribution, dispersibility is preferably；The grain of nano-tungsten powder
For diameter between 12-43 nm, average grain diameter is 27 nm.
Claims (7)
1. a kind of method that DC arc plasma prepares refractory metal nano powder, which is characterized in that specific step is as follows:
(1) using pure tungsten stick as cathode, metal bar of the fusing point higher than 1650 DEG C is anode；
(2) reaction chamber is vacuumized, then passes to plasma gas, setting electric current and voltage carry out arc discharge, same to time control
It is 1 ~ 3 mm that anode processed, which at the uniform velocity rises and controls electric arc spacing,；
(3) step (2) arc discharge terminates, and is passed through passivation gas and is passivated processing, collects the metal nano of reaction chamber wall
Powder.
2. the method that DC arc plasma prepares refractory metal nano powder according to claim 1, it is characterised in that: step
Suddenly (1) anode is tungsten bar, molybdenum bar or stud.
3. the method that DC arc plasma prepares refractory metal nano powder according to claim 1, it is characterised in that: step
Suddenly the diameter of (1) cathode is 10 ~ 20 mm, and 10 ~ 30 cm of length, the bottom end of cathode is cone structure.
4. the method that DC arc plasma prepares refractory metal nano powder according to claim 3, it is characterised in that: step
Suddenly the diameter of (1) anode is 10 ~ 20 mm, 10 ~ 30 cm of length.
5. the method that DC arc plasma prepares refractory metal nano powder according to claim 1, it is characterised in that: step
Suddenly (2) plasma gas is Ar/H2、N2/H2Or He/H2Gaseous mixture system, plasma gas gross pressure are 60 ~ 80 kPa,
H in plasma gas2Volume account for 1/3 ~ 1/2.
6. the method that DC arc plasma prepares refractory metal nano powder according to claim 5, it is characterised in that: step
Suddenly (2) electric current is 150-200 A, and voltage is 25-36 V, and the time of arc discharge is 5-10 min.
7. the method that DC arc plasma prepares refractory metal nano powder according to claim 1, it is characterised in that: step
Suddenly (3) passivation gas is the air of 5 ~ 15 kPa, and passivation time is 8 ~ 10 h.
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Cited By (8)
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| CN111250720A (en) * | 2020-03-02 | 2020-06-09 | 合肥尚德新材料有限公司 | Method for preparing tungsten-copper composite material |
| CN111872407A (en) * | 2020-07-27 | 2020-11-03 | 北华大学 | Preparation method of carbon-coated noble metal ultrafine nanoparticles and product thereof |
| CN112250048A (en) * | 2020-10-28 | 2021-01-22 | 昆明理工大学 | Preparation method of high-purity nano aluminum nitride |
| CN112387979A (en) * | 2020-10-14 | 2021-02-23 | 宁波中乌新材料产业技术研究院有限公司 | Preparation method of silver nanoparticles |
| CN112496333A (en) * | 2020-11-26 | 2021-03-16 | 大连理工大学 | Preparation method and application of Si-Ti alloy nano powder |
| CN113005310A (en) * | 2021-02-23 | 2021-06-22 | 昆明理工大学 | Method for integrating purification of rare earth metal gadolinium and preparation of gadolinium oxide nano material by arc plasma method |
| CN114192793A (en) * | 2021-12-28 | 2022-03-18 | 河北京东管业有限公司 | Spheroidizing process for refractory metal powder |
| US11473171B1 (en) | 2022-05-31 | 2022-10-18 | Kunming University Of Science And Technology | Integrated method for purifying metal gadolinium and preparing gadolinium oxide nanomaterials by arc plasma |
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| CN111250720A (en) * | 2020-03-02 | 2020-06-09 | 合肥尚德新材料有限公司 | Method for preparing tungsten-copper composite material |
| CN111250720B (en) * | 2020-03-02 | 2023-02-28 | 合肥尚德新材料有限公司 | Method for preparing tungsten-copper composite material |
| CN111872407A (en) * | 2020-07-27 | 2020-11-03 | 北华大学 | Preparation method of carbon-coated noble metal ultrafine nanoparticles and product thereof |
| CN111872407B (en) * | 2020-07-27 | 2022-12-27 | 北华大学 | Preparation method of carbon-coated noble metal ultrafine nanoparticles and product thereof |
| CN112387979A (en) * | 2020-10-14 | 2021-02-23 | 宁波中乌新材料产业技术研究院有限公司 | Preparation method of silver nanoparticles |
| CN112250048A (en) * | 2020-10-28 | 2021-01-22 | 昆明理工大学 | Preparation method of high-purity nano aluminum nitride |
| CN112496333A (en) * | 2020-11-26 | 2021-03-16 | 大连理工大学 | Preparation method and application of Si-Ti alloy nano powder |
| CN113005310A (en) * | 2021-02-23 | 2021-06-22 | 昆明理工大学 | Method for integrating purification of rare earth metal gadolinium and preparation of gadolinium oxide nano material by arc plasma method |
| CN114192793A (en) * | 2021-12-28 | 2022-03-18 | 河北京东管业有限公司 | Spheroidizing process for refractory metal powder |
| CN114192793B (en) * | 2021-12-28 | 2023-07-21 | 河北京东管业有限公司 | Spheroidizing process for refractory metal powder |
| US11473171B1 (en) | 2022-05-31 | 2022-10-18 | Kunming University Of Science And Technology | Integrated method for purifying metal gadolinium and preparing gadolinium oxide nanomaterials by arc plasma |
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